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Methanol → HCID 21474716、化合物

HRID 2294292
ノート
印刷プレビュー

反応式

HRID 2294292 の反応式
[BH4-].[Li+].[Cl:3][C:4]1[CH:5]=[C:6]([CH:22]=[CH:23][CH:24]=1)[O:7][CH2:8][CH:9]1[O:13][C:12](=[O:14])[N:11]([CH:15]([CH3:21])[C:16](OCC)=[O:17])[CH2:10]1.CO>O1CCCC1>[Cl:3][C:4]1[CH:5]=[C:6]([CH:22]=[CH:23][CH:24]=1)[O:7][CH2:8][CH:9]1[O:13][C:12](=[O:14])[N:11]([CH:15]([CH3:21])[CH2:16][OH:17])[CH2:10]1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 887MethanolHCID 4148881Lithium borohydrideHCID 21474732HCID 21474732、化合物

生成物 1

HCID 21474716HCID 21474716、化合物収率 36.2%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

0.4 g of lithium borohydride was added, whilst ice-cooling, to a solution of 2.95 g of ethyl 2-[5-(3-chlorophenoxymethyl)-2-oxooxazolidin-3-yl]propionate (prepared as described in Preparation 4) in 25 ml of tetrahydrofuran, and then a mixture of 0.37 ml of methanol and 5 ml of tetrahydrofuran was added dropwise to the resulting mixture. The reaction mixture was then stirred at room temperature for 2 hours. At the end of this time, the tetrahydrofuran was removed from the reaction mixture by evaporation under reduced pressure, and an aqueous solution of sodium chloride was added to the resulting residue, which was then extracted with ethyl acetate. The extract was dried over anhydrous sodium sulfate. The ethyl acetate was then removed from the extract by evaporation under reduced pressure, and the resulting residue was recrystallized from ethyl acetate, to give 0.93 g of the title compound, melting at 114° C. to 115° C.

後処理

  1. additionwas added dropwise to the resulting mixture
  2. customAt the end of this time, the tetrahydrofuran was removed from the reaction mixture by evaporation under reduced pressure
  3. additionan aqueous solution of sodium chloride was added to the resulting residue, which
  4. extractionwas then extracted with ethyl acetate
  5. dry with materialThe extract was dried over anhydrous sodium sulfate
  6. customThe ethyl acetate was then removed from the
  7. extractionextract by evaporation under reduced pressure
  8. customthe resulting residue was recrystallized from ethyl acetate

出典と根拠

ORDレコード
ord-c8d4307f0c6644c68c6d77e34ab0ee60
出典データセット
uspto-grants-1997_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05688823

反応ノート

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